Researchers who often do experiments know that organic synthesis is a process of preparing more complex target molecules from simple raw materials through one or more chemical reactions. Generally, it requires fewer steps, and cheap raw materials. 1189352-83-7, name is 3-Chloro-5-iodobenzotrifluoride, A new synthetic method of this compound is introduced below., Formula: C7H3ClF3I
2)9- (4-methoxyphenyl) -10 anthracene boronate 3mmol,1-chloro-3-iodo-5-trifluoromethyl-4,6-dihydrosubstituted benzene 3 mmol,Tetrakis(triphenylphosphine)palladium 0.3 mmol,Toluene 120mL,30 mL of ethanol and 120 mmol of K2CO3 (formed as a solution with 30 mL of distilled water) were added to the reaction flask.Then vacuum the system,Nitrogen protection,The reaction was carried out at 110 C for 24 hours.After the reaction,extraction,Rotary evaporation,Column chromatography (eluent: n-hexane / dichloromethane = 1:1),Recrystallization gave the product A9.The yield was 69%. 3)Will A9 2mmol,Boronic acid pinacol ester 6mmol,Palladium acetate 0.2 mmol,2-dicyclohexylphosphine-2′,6′-dimethoxybiphenyl 0.4 mmol,Potassium acetate 6mmol,Add 1,4-dioxane 90mL to the reaction flask,Then vacuum the system,Nitrogen protection,The reaction was carried out at 105 C for 18 hours.After the reaction,extraction,Rotary evaporation,Column chromatography (eluent: n-hexane / dichloromethane = 2:1),Recrystallization to give the product B9,The yield was 68%. 4)The final product i is obtained by Suzuki coupling reaction: B9 1mmol,The product obtained in step 2 is 9-bromo-10-(4-cyano)benzoquinone 0.84 mmol.Catalyst tetrakis(triphenyl)phosphine palladium 0.12 mmol,Toluene 60mL,20mL of ethanol,K2CO3 33.6mmol (formed into solution with 20mL distilled water),Add to the reaction bottle,Under the protection of nitrogen,It was refluxed at 110 C for 24 h.After the reaction, the methanol is hot washed,Filtering,Recrystallization of toluene,Sublimation gives the final product.The yield was 69%.
The basis of chemical reaction formula synthesis, the synthesis route is composed of some specific reactions and combined according to certain logical thinking. We look forward to the emergence of more reaction modes in the future.
Reference:
Patent; Shaanxi Normal University; Hu Jianyong; Zhang Jiali; Zhao Zhen; Duan Xuewei; (24 pag.)CN109503427; (2019); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com